CN116237225A - High-sensitivity flexible piezoelectric ultrasonic transducer and preparation method thereof - Google Patents
High-sensitivity flexible piezoelectric ultrasonic transducer and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B06—GENERATING OR TRANSMITTING MECHANICAL VIBRATIONS IN GENERAL
- B06B—METHODS OR APPARATUS FOR GENERATING OR TRANSMITTING MECHANICAL VIBRATIONS OF INFRASONIC, SONIC, OR ULTRASONIC FREQUENCY, e.g. FOR PERFORMING MECHANICAL WORK IN GENERAL
- B06B1/00—Methods or apparatus for generating mechanical vibrations of infrasonic, sonic, or ultrasonic frequency
- B06B1/02—Methods or apparatus for generating mechanical vibrations of infrasonic, sonic, or ultrasonic frequency making use of electrical energy
- B06B1/06—Methods or apparatus for generating mechanical vibrations of infrasonic, sonic, or ultrasonic frequency making use of electrical energy operating with piezoelectric effect or with electrostriction
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Abstract
The invention discloses a high-sensitivity flexible piezoelectric ultrasonic transducer and a preparation method thereof, and belongs to the technical field of flexible sensors. The piezoelectric ultrasonic transducer comprises a flexible substrate with a cavity structure, an elastic layer, a bottom electrode, a piezoelectric layer, an upper electrode and an insulating layer which are sequentially arranged, wherein the piezoelectric layer is made of a piezoelectric material Ba 0.92 Ca 0.08 Ti 1‑x Sn x O 3 The thin film, x is 0.01-0.1, has high-voltage electrical property and pollution-free advantage, the elastic layer is a high-temperature resistant white mica sheet, and is compatible with a microelectronic process and a piezoelectric material high-temperature annealing process. The piezoelectric ultrasonic transducer provided by the invention integrates ultrasonic transmitting and receiving functions, has small size and can be deformed greatly, and is suitable for the fields of non-planar structure nondestructive inspection, biological tissue imaging, human body wearable equipment and the like. The high-sensitivity flexible piezoelectric ultrasonic transducer disclosed by the invention has the advantages of simple preparation method and low cost, and is suitable for mass production.
Description
Technical Field
The invention relates to the technical field of flexible sensors, in particular to a high-sensitivity flexible piezoelectric ultrasonic transducer and a preparation method thereof.
Background
The ultrasonic transducer has wide application in the fields of biomedical imaging, industrial nondestructive detection, ocean exploration and the like. However, the characteristics of fixed shape and non-deformability of the conventional rigid ultrasonic transducer are difficult to realize close fitting with biological tissues and structures to be tested with arbitrary shapes/contours, so that the application scenes and the use performance of the transducer are limited.
Flexible ultrasonic transducers have been widely studied in recent years to achieve intimate contact with complex contoured objects. There are two main technical routes for developing flexible ultrasonic transducers:
1) The transfer of transducer structures deposited on silicon substrates to flexible substrates by transfer methods (Transfer Printing) such as those disclosed in Liu tuning in 2021 (Liu t.et al., sensors,2021,21,1014).
The technical method mostly adopts piezoelectric materials with high piezoelectric coefficients, such as PZT, to construct the piezoelectric layer. Although high emission sensitivity can be achieved, lead-containing piezoelectric materials are prone to environmental pollution.
In addition, the technology is complex in process, expensive in experimental equipment and harsh in preparation conditions, so that the yield is low and the cost is high.
2) The piezoelectric material is directly bonded with the flexible substrate, and the method is getting more and more attention by virtue of the advantages of flexibility in operation, low preparation cost and the like. Ranging flexible transducers based on polyvinylidene fluoride (PVDF) were developed as taught by university of aerospace in south kyo Wu Dawei (Liu t.et al, sens. Actator a Phys.,2021,317,112476); the belgium microelectronics research center (IMEC) developed a PVDF-based flexible transducer and enabled gesture recognition (gijsenbergh p.et al., j. Micromech. Micro., 2019,29,074001).
The flexible transducer developed by the method at present adopts piezoelectric organic polymers, such as PVDF (d) 33 -20 pC/N), P (VDF-TrFE) (d 33 30 pC/N), etc., as a piezoelectric layer, the piezoelectric coefficient is low, and it is difficult to achieve high emission sensitivity.
In addition, most of the reported flexible transducer elastic layer materials are polyimide, polyethylene terephthalate, polyvinyl chloride and the like, and are difficult to be compatible with a high-temperature annealing process in the preparation of piezoelectric materials with high piezoelectric coefficients.
Therefore, how to improve the emission sensitivity of the transducer and reduce the complexity of the manufacturing process while achieving the close fitting of the flexible ultrasonic transducer to the complex contour/surface is a problem to be solved by those skilled in the art.
Disclosure of Invention
The invention aims to provide a flexible piezoelectric ultrasonic transducer with high sensitivity and a preparation method thereof, so as to realize the functions of effectively transmitting and receiving ultrasonic waves and meet the requirements of simple preparation process and low cost.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the invention provides a high-sensitivity flexible piezoelectric ultrasonic transducer which comprises a flexible substrate with a cavity structure, an elastic layer, a bottom electrode, a piezoelectric layer, an upper electrode and an insulating layer which are sequentially arranged, wherein the elastic layer is prepared from a white mica sheet, and the piezoelectric layer is Ba 0.92 Ca 0.08 Ti 1-x Sn x O 3 The film, x is 0.01-0.1.
The invention adopts the high-performance environment-friendly piezoelectric material Ba 0.92 Ca 0.08 Ti 1-x Sn x O 3 The piezoelectric layer is prepared, and the material has high piezoelectric coefficient and electromechanical coupling coefficient and high electroacoustic conversion efficiency. The high-temperature-resistant flexible muscovite elastic layer is adopted to adapt to the high-temperature annealing process of the piezoelectric material, and meanwhile, the muscovite has high flexibility, so that the sensitivity of the transducer is improved.
The elastic layer is prepared by grinding and stripping a white mica sheet. Preferably, the elastic layer has a thickness of 10 to 100. Mu.m. More preferably, the thickness of the elastic layer is 30-55 μm, the thickness of the elastic layer influences the quality factor, namely the bandwidth, and the acoustic damping can be properly increased under the thickness condition, so that the bandwidth of the transducer is improved.
The piezoelectric layer is made of Ba 0.92 Ca 0.08 Ti 1-x Sn x O 3 The sol is dripped on the surface of the bottom electrode, and is formed after spin coating, baking and annealing. The Ba is 0.92 Ca 0.08 Ti 1-x Sn x O 3 The preparation method of the sol comprises the following steps: barium titanate, calcium carbonate, titanium dioxide and tin dioxide powder are mixed according to a stoichiometric ratio of 92:8:100-100x:100x (x is 0.01-0.1) is mixed and dissolved in absolute ethyl alcohol, and the mixture is fully mixed and ball-milled to prepare slurry; however, the method is thatDrying the obtained slurry, and calcining in 1200-1400 ℃ environment to prepare Ba 0.92 Ca 0.08 Ti 1-x Sn x O 3 The method comprises the steps of carrying out a first treatment on the surface of the Ba is added to 0.92 Ca 0.08 Ti 1-x Sn x O 3 Dissolving in absolute ethanol to obtain Ba 0.92 Ca 0.08 Ti 1-x Sn x O 3 And (3) sol.
Preferably, the piezoelectric layer material is Ba 0.92 Ca 0.08 Ti 0.98 Sn 0.02 O 3 、Ba 0.92 Ca 0.08 Ti 0.96 Sn 0.04 O 3 Or Ba (Ba) 0.92 Ca 0.08 Ti 0.95 Sn 0.05 O 3 。
Preferably, the thickness of the piezoelectric layer is 0.5 to 10 μm. Furthermore, the thickness of the piezoelectric layer is 1-5 mu m, and the piezoelectric layer with the thickness is easy to prepare and can improve the emission sensitivity of the transducer; more preferably, the thickness of the piezoelectric layer is 1 to 2. Mu.m.
Preferably, the flexible substrate is prepared from a polydimethylsiloxane film, and the depth of the cavity is 100-500 mu m. The depth of the cavity affects the stress distribution, more preferably the depth of the cavity is 200-300 μm, to improve the uniformity of the stress distribution and improve the overall performance of the transducer. The cavity inner diameter is 100-250 μm, preferably 130-225 μm.
Preferably, the bottom electrode and the upper electrode are both titanium-platinum films, wherein the thickness of the titanium film layer is 10-50 nm, and the thickness of the platinum film layer is 100-300 nm. Preferably, the thickness of the titanium film layer in the bottom electrode is 20-30 nm, and the thickness of the platinum film layer is 200-300 nm; the thickness of the titanium film layer in the upper electrode is 10-20 nm, and the thickness of the platinum film layer is 150-180 nm. Specifically, the thickness of the titanium film layer in the bottom electrode is 20nm, the thickness of the platinum film layer is 300nm, the thickness of the titanium film layer in the upper electrode is 10nm, and the thickness of the platinum film layer is 150nm; or the thickness of the titanium film layer in the bottom electrode is 25nm, the thickness of the platinum film layer in the upper electrode is 250nm, the thickness of the titanium film layer in the bottom electrode is 15nm, and the thickness of the platinum film layer in the upper electrode is 175nm; or the thickness of the titanium film layer in the bottom electrode is 30nm, the thickness of the platinum film layer in the upper electrode is 200nm, and the thickness of the titanium film layer in the upper electrode is 20nm, and the thickness of the platinum film layer is 180nm.
Preferably, the insulating layer is a silicon nitride film with the thickness of 0.5-5 μm and is used for water resistance, dust prevention and corrosion resistance. More preferably, the insulating layer has a thickness of 1 to 2. Mu.m.
The invention also provides a method for preparing the high-sensitivity flexible piezoelectric ultrasonic transducer, which comprises the following steps:
(1) Taking a white mica sheet, and grinding and stripping the white mica sheet to obtain an elastic layer;
(2) Sequentially preparing a bottom electrode, a piezoelectric layer, an upper electrode and an insulating layer on the upper surface of the elastic layer, wherein the piezoelectric layer is composed of Ba 0.92 Ca 0.08 Ti 1-x Sn x O 3 Dripping sol on the surface of the bottom electrode, and performing spin coating, baking and annealing to form the electrode;
(3) And taking a Polydimethylsiloxane (PDMS) film as a flexible substrate material, etching the middle area of the flexible substrate by adopting a photolithography method to form a cavity structure, bonding the prepared flexible substrate and the lower surface of the elastic layer by adopting a hot pressing method, and covering the cavity of the flexible substrate by the elastic layer.
In the step (2), a direct current magnetron sputtering method is adopted to deposit a titanium film and a platinum film on the upper surface of the elastic layer to form a bottom electrode, then a piezoelectric material is spin-coated on the surface of the bottom electrode, the piezoelectric layer is formed through an annealing process, then the direct current magnetron sputtering method is adopted to deposit the titanium film and the platinum film on the surface of the piezoelectric layer to form an upper electrode, and finally an insulating layer is prepared on the surface of the upper electrode.
The Ba is 0.92 Ca 0.08 Ti 1-x Sn x O 3 The preparation method of the sol comprises the following steps: barium titanate, calcium carbonate, titanium dioxide and tin dioxide powder are mixed according to a stoichiometric ratio of 92:8:100-100x:100x (x is 0.01-0.1) is mixed and dissolved in absolute ethyl alcohol, and fully mixed and ball-milled for 12-24 hours; then the obtained slurry is put into an environment of 80-100 ℃ to be baked for 6-12 hours; calcining the dried slurry at 1200-1400 ℃ for 2-6 hours to prepare Ba 0.92 Ca 0.08 Ti 1-x Sn x O 3 The method comprises the steps of carrying out a first treatment on the surface of the Ba is added to 0.92 Ca 0.08 Ti 1-x Sn x O 3 Dissolving in absolute ethanol to obtain Ba 0.92 Ca 0.08 Ti 1-x Sn x O 3 And (3) sol.
Preferably, in the process of preparing the piezoelectric layer, the baking temperature is 150-350 ℃ and the duration time is 2-10 minutes; the annealing temperature is 450-1300 ℃ and the duration time is 2-30 minutes. More preferably, the baking temperature is 200-300 ℃ and the duration is 2-6 minutes; the annealing temperature is 1000-1200 ℃ and the duration time is 10-15 minutes.
Preferably, in the step (2) of the preparation method, the insulating layer is a silicon nitride film, silicon nitride is grown on the upper electrode by adopting a chemical vapor deposition method, the air pressure is 500-1000 mTorr, the temperature is 300-500 ℃, and the reaction gas SiH 4 With NH 3 The proportion is 1:0.5 to 1, the reaction gas SiH 4 And N 2 The proportion is 1:10 to 20. More preferably, the chemical vapor deposition method adopts the gas pressure of 500-800 mTorr, the temperature of 300-450 ℃ and the reaction gas SiH 4 With NH 3 The proportion is 1:0.5 to 0.6, the reaction gas SiH 4 And N 2 The proportion is 1: 15-20.
In the step (3), a cavity structure of the flexible substrate is prepared by an etching method, and then the flexible substrate is bonded on the lower surface of the elastic layer by a hot pressing method, and the cavity of the PDMS substrate is covered by the white mica sheet.
Preferably, the photolithography method includes: and dry etching is carried out on the middle area of the PDMS organic silicon film by taking photoresist as a mask, wherein the step is carried out in a low-temperature inductively coupled plasma etching system, and the etching parameters are as follows: 100% SF 6 The flow rate is 100-300 sccm, the power is 1200-2000W, the pressure is 0.01-0.03 mbar, the etching time is 30-60 minutes, and finally the cavity structure is formed. More preferably, the etching parameters are as follows: 100% SF 6 The flow rate is 150-200 sccm, the power is 1200-1800W, the pressure is 0.01-0.02 mbar, and the etching time is 30-40 minutes.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention adopts the high-temperature-resistant flexible white mica sheet as the elastic layer, and is compatible with a microelectronic process and a piezoelectric material high-temperature annealing process.
(2) The invention adopts the lead-free piezoelectric material Ba with high piezoelectric coefficient 0.92 Ca 0.08 Ti 1-x Sn x O 3 (d 33 400-600 pC/N, d 31 -500 to-200 pC/N) to achieve high emission sensitivity, doping appropriate amount of Sn to enhance piezoelectric properties, and at the same time, increasing crystal ductility and effectively reducing annealing temperature, and also avoiding environmental pollution.
(3) The preparation method is simple, suitable for mass production, high in yield and low in cost, and an inefficient and complicated transfer printing method is not required.
(4) The flexible transducer provided by the invention has small size and can be deformed greatly, and has wide application prospects in the fields of non-planar structure nondestructive inspection, organism tissue imaging, human body wearable equipment and the like.
Drawings
Fig. 1 is a schematic diagram of the overall design of a high-sensitivity flexible piezoelectric ultrasonic transducer.
In the figure, 1-flexible substrate (containing cavity); 2-an elastic layer of white mica sheet; 3-titanium bottom electrode; a 4-platinum bottom electrode; 5-piezoelectric layer Ba 0.92 Ca 0.08 Ti 1-x Sn x O 3 A film; a 6-titanium upper electrode; a 7-platinum upper electrode; 8-silicon nitride insulating layer, the same applies below.
Fig. 2 is a flowchart of a preparation method of a high-sensitivity flexible piezoelectric ultrasonic transducer, which sequentially comprises the steps of grinding and stripping to prepare a white mica sheet elastic layer, depositing a titanium film layer on the upper surface of the white mica sheet, depositing a platinum film layer on the titanium film, spin-coating a piezoelectric material on the platinum film layer, forming the piezoelectric layer through an annealing process, depositing a titanium film on the surface of the piezoelectric layer, depositing a platinum film layer on the titanium film, preparing an insulating layer on the surface of the platinum film layer, taking a PDMS organic silicon film as a flexible substrate material, forming a cavity structure in the middle area by adopting an etching method, and bonding the prepared PDMS substrate with the lower surface of the white mica sheet by adopting a hot pressing method.
FIG. 3 is a schematic representation of the emission sensitivity of a 500kHz transducer prepared in accordance with the embodiment 1 of the present invention.
FIG. 4 is a schematic diagram of the emission sensitivity of a 2MHz transducer prepared according to scheme 2 of the present invention.
FIG. 5 is a schematic diagram of the emission sensitivity of a 3MHz transducer prepared according to embodiment 3 of the present invention.
Detailed Description
The invention will be further illustrated with reference to specific examples. The following examples are only for illustrating the present invention, and are not intended to limit the scope of the present invention, and the technical features of the various embodiments of the present invention can be combined correspondingly without conflicting with each other. Modifications and substitutions to methods, procedures, or conditions of the present invention without departing from the spirit and nature of the invention are intended to be within the scope of the present invention.
The test methods used in the following examples are conventional methods unless otherwise specified; the materials, reagents and the like used, unless otherwise specified, are those commercially available.
PDMS silicone films were purchased from Gui Zhu, white mica flakes were purchased from Nanjing Michata photovoltaic Co. Piezoelectric material Ba 0.92 Ca 0.08 Ti 1-x Sn x O 3 From barium titanate (BaTiO) 3 ) Titanium dioxide (TiO) 2 ) Calcium carbonate (CaCO) 3 ) Tin dioxide (SnO) 2 ) Mixing, grinding and calcining according to a specific stoichiometric ratio; the above barium titanate, titanium dioxide, calcium carbonate, and tin dioxide were all purchased from Sigma-Aldrich.
Example 1
As shown in fig. 1, the present embodiment provides a high-sensitivity flexible piezoelectric ultrasonic transducer, which structurally comprises a flexible substrate 1 with a cavity structure, an elastic layer 2, a bottom electrode (composed of a titanium bottom electrode 3 and a platinum bottom electrode 4), a piezoelectric layer 5, an upper electrode (composed of a titanium upper electrode 6 and a platinum upper electrode 7) and an insulating layer 8, which are sequentially arranged.
Specifically, the flexible substrate 1 is made of Polydimethylsiloxane (PDMS), and has a cavity structure, wherein the depth of the cavity is 300 μm, and the inner diameter is 225 μm. The elastic layer 2 is a high temperature resistant white mica sheet with a thickness of 30 μm. The bottom electrode is a titanium-platinum film, wherein the thickness of the titanium film is 20nm, and the thickness of the platinum film300nm; the upper electrode is a titanium-platinum film, wherein the thickness of the titanium film is 10nm, and the thickness of the platinum film is 150nm. The piezoelectric layer 5 is made of Ba 0.92 Ca 0.08 Ti 0.98 Sn 0.02 O 3 The thickness was 1. Mu.m. The insulating layer 8 is a silicon nitride film having a thickness of 1 μm.
1. Preparation method
1) Barium titanate (BaTiO) 3 ) Calcium carbonate (CaCO) 3 ) Titanium dioxide (TiO) 2 ) Tin dioxide (SnO) 2 ) Powder in stoichiometric ratio 92:8:98:2, mixing and dissolving in absolute ethyl alcohol, fully mixing and ball milling for 12 hours; baking the obtained slurry in an environment of 80 ℃ for 12 hours; calcining the dried slurry at 1200 ℃ for 6 hours to prepare Ba 0.92 Ca 0.08 Ti 0.98 Sn 0.02 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Ba is added to 0.92 Ca 0.08 Ti 0.98 Sn 0.02 O 3 Dissolving in absolute ethanol to obtain Ba 0.92 Ca 0.08 Ti 0.98 Sn 0.02 O 3 And (3) sol.
2) The white mica sheet was taken and subjected to grinding and peeling treatment to obtain an elastic layer having a thickness of 30. Mu.m.
3) Preparing a bottom electrode titanium-platinum film, firstly taking pure titanium as a target material, and adopting a direct-current magnetron sputtering method to deposit a titanium film on the surface of a flexible white mica sheet, wherein the thickness of the titanium film is 20nm; and then, using pure platinum as a target material, and adopting a direct-current magnetron sputtering method to deposit a platinum film on the surface of the titanium film, wherein the thickness is 300nm.
4) Ba is added to 0.92 Ca 0.08 Ti 0.98 Sn 0.02 O 3 Spin-coating sol on the surface of the bottom electrode for spin-coating, and controlling the thickness of the piezoelectric thin film to be 1 mu m through repeating the spin-coating process for a plurality of times; then baking at 200 ℃ for 2 minutes; finally, annealing was performed at 1000℃for 15 minutes.
5) Preparing an upper electrode titanium-platinum film, namely firstly taking pure titanium as a target material, and adopting a direct-current magnetron sputtering method to deposit the titanium film on the surface of the piezoelectric layer, wherein the thickness is 10nm; and then, using pure platinum as a target material, and adopting a direct-current magnetron sputtering method to deposit a platinum film on the surface of the titanium film, wherein the thickness is 150nm.
6) Silicon nitride grows on the surface of the upper electrode by adopting a chemical vapor deposition method, silane and ammonia are respectively used as a silicon source and a nitrogen source of a silicon nitride film by adopting the chemical vapor deposition method, and high-purity nitrogen is used as carrier gas, and the preparation conditions are as follows: the gas pressure is 500mTorr, the temperature is 300 ℃, and the reaction gas SiH 4 With NH 3 The proportion is 1:0.5, reaction gas SiH 4 And N 2 The proportion is 1:15.
7) Taking a PDMS organic silicon film as a flexible substrate material, and adopting a photoresist AZ4620 as a mask to carry out dry etching on a middle area of the flexible substrate material, wherein the step is carried out in a low-temperature inductively coupled plasma etching system, and the etching parameters are as follows: 100% SF 6 The flow rate is 150sccm, the power is 1200W, the pressure is 0.01mbar, the etching time is 40 minutes, and finally the cavity structure is formed. And then aligning the prepared flexible PDMS substrate with the white mica sheet, and bonding the PDMS substrate to the lower surface of the white mica sheet by adopting a hot pressing method.
The working principle of the high-sensitivity flexible piezoelectric ultrasonic transducer is as follows:
the high-sensitivity flexible piezoelectric ultrasonic transducer prepared by the embodiment has the function of transmitting and receiving ultrasonic waves. When ultrasonic waves are emitted, an electric field between the upper electrode and the bottom electrode causes the piezoelectric layer to produce an inverse piezoelectric effect, thereby producing transverse stress in the piezoelectric layer. Due to the bottom constraint, the stress generates a bending moment, forcing the membrane out of plane, and transmitting ultrasonic waves to the surrounding medium. When receiving ultrasonic waves, the pressure waves deflect the plate to create lateral stresses, and the piezoelectric layer creates an electrical charge on the electrodes by virtue of the piezoelectric effect. The invention adopts the lead-free piezoelectric material Ba with high piezoelectric coefficient 0.92 Ca 0.08 Ti 1-x Sn x O 3 (d 33 400-600 pC/N, d 31 -500 to-200 pC/N) to achieve high emission sensitivity, doping appropriate amount of Sn to enhance piezoelectric performance; the invention also adopts the high temperature resistant white mica sheet as the elastic layer, has high flexibility and is beneficial to improving the sensitivity of the transducer.
2. Performance testing
The prepared flexible piezoelectric ultrasonic transducer is tested to obtain the emission sensitivity schematic diagram shown in figure 3, the center frequency is 500kHz, the emission sensitivity is 1650Pa/V, and the performance of the flexible piezoelectric ultrasonic transducer exceeds that of the reported flexible transducer (generally less than 1000 Pa/V).
Example 2
As shown in fig. 1, the present embodiment provides a high-sensitivity flexible piezoelectric ultrasonic transducer, which structurally comprises a flexible substrate 1 with a cavity structure, an elastic layer 2, a bottom electrode (composed of a titanium bottom electrode 3 and a platinum bottom electrode 4), a piezoelectric layer 5, an upper electrode (composed of a titanium upper electrode 6 and a platinum upper electrode 7) and an insulating layer 8, which are sequentially arranged.
Specifically, the flexible substrate 1 is made of Polydimethylsiloxane (PDMS), and has a cavity structure, wherein the depth of the cavity is 250 μm, and the inner diameter is 150 μm. The elastic layer 2 is a high temperature resistant white mica sheet with a thickness of 50 μm. The bottom electrode is a titanium-platinum film, wherein the thickness of the titanium film is 25nm, and the thickness of the platinum film is 250nm; the upper electrode is a titanium-platinum film, wherein the thickness of the titanium film is 15nm, and the thickness of the platinum film is 175nm. The piezoelectric layer 5 is made of Ba 0.92 Ca 0.08 Ti 0.96 Sn 0.04 O 3 The thickness was 1.5. Mu.m. The insulating layer 8 is a silicon nitride film having a thickness of 1.5 μm.
1. Preparation method
1) Barium titanate (BaTiO) 3 ) Calcium carbonate (CaCO) 3 ) Titanium dioxide (TiO) 2 ) Tin dioxide (SnO) 2 ) Powder in stoichiometric ratio 92:8:96:4, mixing and dissolving in absolute ethyl alcohol, fully mixing and ball milling for 18 hours; the obtained slurry is placed in a 90 ℃ environment for baking for 9 hours; calcining the dried slurry at 1300 ℃ for 4 hours to prepare Ba 0.92 Ca 0.08 Ti 0.96 Sn 0.04 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Ba is added to 0.92 Ca 0.08 Ti 0.96 Sn 0.04 O 3 Dissolving in absolute ethanol to obtain Ba 0.92 Ca 0.08 Ti 0.96 Sn 0.04 O 3 And (3) sol.
2) The white mica sheet was taken and subjected to grinding and peeling treatment to obtain an elastic layer having a thickness of 50. Mu.m.
3) Preparing a bottom electrode titanium-platinum film, firstly taking pure titanium as a target material, and adopting a direct-current magnetron sputtering method to deposit a titanium film on the surface of a flexible white mica sheet, wherein the thickness is 25nm; and then, using pure platinum as a target material, and adopting a direct-current magnetron sputtering method to deposit a platinum film on the surface of the titanium film, wherein the thickness is 250nm.
4) Ba is added to 0.92 Ca 0.08 Ti 0.96 Sn 0.04 O 3 Spin-coating sol on the surface of the bottom electrode for spin-coating, and controlling the thickness of the piezoelectric thin film to be 1.5 mu m through repeating the spin-coating process for a plurality of times; then baking at 250 ℃ for 5 minutes; finally, annealing was performed at 1150℃for 13 minutes.
5) Preparing an upper electrode titanium-platinum film, firstly taking pure titanium as a target material, and adopting a direct current magnetron sputtering method to deposit the titanium film on the surface of the piezoelectric layer, wherein the thickness is 15nm; and then, pure platinum is used as a target material, and a direct-current magnetron sputtering method is adopted to deposit a platinum film on the surface of the titanium film, wherein the thickness of the platinum film is 175nm.
6) Silicon nitride grows on the surface of the upper electrode by adopting a chemical vapor deposition method, silane and ammonia are respectively used as a silicon source and a nitrogen source of a silicon nitride film by adopting the chemical vapor deposition method, and high-purity nitrogen is used as carrier gas, and the preparation conditions are as follows: the gas pressure is 600mTorr, the temperature is 400 ℃, and the reaction gas SiH 4 With NH 3 The proportion is 1:0.55, reaction gas SiH 4 And N 2 The proportion is 1:18.
7) Taking a PDMS organic silicon film as a flexible substrate material, and adopting a photoresist AZ4620 as a mask to carry out dry etching on a middle area of the flexible substrate material, wherein the step is carried out in a low-temperature inductively coupled plasma etching system, and the etching parameters are as follows: 100% SF 6 The flow rate is 150sccm, the power is 1800W, the pressure is 0.015mbar, the etching time is 35 minutes, and finally the cavity structure is formed. And then aligning the prepared flexible PDMS substrate with the white mica sheet, and bonding the PDMS substrate to the lower surface of the white mica sheet by adopting a hot pressing method.
2. Performance testing
The prepared flexible piezoelectric ultrasonic transducer is tested to obtain a transmission sensitivity schematic diagram shown in fig. 4, the center frequency is 2MHz, the transmission sensitivity is 1500Pa/V, and the transmission sensitivity exceeds the reported performance (generally less than 1000 Pa/V) of the flexible transducer.
Example 3
As shown in fig. 1, the present embodiment provides a high-sensitivity flexible piezoelectric ultrasonic transducer, which structurally comprises a flexible substrate 1 with a cavity structure, an elastic layer 2, a bottom electrode (composed of a titanium bottom electrode 3 and a platinum bottom electrode 4), a piezoelectric layer 5, an upper electrode (composed of a titanium upper electrode 6 and a platinum upper electrode 7) and an insulating layer 8, which are sequentially arranged.
Specifically, the flexible substrate 1 is made of Polydimethylsiloxane (PDMS), and has a cavity structure, wherein the depth of the cavity is 200 μm, and the inner diameter is 130 μm. The elastic layer 2 is a high temperature resistant white mica sheet with a thickness of 55 μm. The bottom electrode is a titanium-platinum film, wherein the thickness of the titanium film is 30nm, and the thickness of the platinum film is 200nm; the upper electrode is a titanium-platinum film, wherein the thickness of the titanium film is 20nm, and the thickness of the platinum film is 180nm. The piezoelectric layer 5 is made of Ba 0.92 Ca 0.08 Ti 0.95 Sn 0.05 O 3 The thickness was 2. Mu.m. The insulating layer 8 is a silicon nitride film having a thickness of 2 μm.
1. Preparation method
1) Barium titanate (BaTiO) 3 ) Calcium carbonate (CaCO) 3 ) Titanium dioxide (TiO) 2 ) Tin dioxide (SnO) 2 ) Powder in stoichiometric ratio 92:8:95:5, mixing and dissolving in absolute ethyl alcohol, fully mixing and ball milling for 24 hours; the obtained slurry is placed in an environment of 80-100 ℃ and baked for 6 hours; calcining the dried slurry at 1400 ℃ for 2 hours to prepare Ba 0.92 Ca 0.08 Ti 0.95 Sn 0.05 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Ba is added to 0.92 Ca 0.08 Ti 0.95 Sn 0.05 O 3 Dissolving in absolute ethanol to obtain Ba 0.92 Ca 0.08 Ti 0.95 Sn 0.05 O 3 And (3) sol.
2) The white mica sheet was taken and subjected to grinding and peeling treatment to obtain an elastic layer having a thickness of 55. Mu.m.
3) Preparing a bottom electrode titanium-platinum film, firstly taking pure titanium as a target material, and adopting a direct-current magnetron sputtering method to deposit a titanium film on the surface of a flexible white mica sheet, wherein the thickness is 30nm; and then, using pure platinum as a target material, and adopting a direct-current magnetron sputtering method to deposit a platinum film on the surface of the titanium film, wherein the thickness is 200nm.
4) Ba is added to 0.92 Ca 0.08 Ti 0.95 Sn 0.05 O 3 Spin-coating the sol on the surface of the bottom electrode for spin-coating, and controlling the thickness of the piezoelectric film to be 2 mu m through repeating the spin-coating process for a plurality of times; then baking at 300 ℃ for 6 minutes; finally, annealing was performed at 1200 ℃ for 10 minutes.
5) Preparing an upper electrode titanium-platinum film, namely firstly taking pure titanium as a target material, and adopting a direct-current magnetron sputtering method to deposit the titanium film on the surface of the piezoelectric layer, wherein the thickness of the titanium film is 20nm; and then, using pure platinum as a target material, and adopting a direct-current magnetron sputtering method to deposit a platinum film on the surface of the titanium film, wherein the thickness is 180nm.
6) Silicon nitride grows on the surface of the upper electrode by adopting a chemical vapor deposition method, silane and ammonia are respectively used as a silicon source and a nitrogen source of a silicon nitride film by adopting the chemical vapor deposition method, and high-purity nitrogen is used as carrier gas, and the preparation conditions are as follows: the gas pressure is 800mTorr, the temperature is 450 ℃, and the reaction gas SiH 4 With NH 3 The proportion is 1:0.6, reaction gas SiH 4 And N 2 The proportion is 1:20.
7) Taking a PDMS organic silicon film as a flexible substrate material, and adopting a photoresist AZ4620 as a mask to carry out dry etching on a middle area of the flexible substrate material, wherein the step is carried out in a low-temperature inductively coupled plasma etching system, and the etching parameters are as follows: 100% SF 6 The flow rate is 200sccm, the power is 1500W, the pressure is 0.02mbar, the etching time is 30 minutes, and finally the cavity structure is formed. And then aligning the prepared flexible PDMS substrate with the white mica sheet, and bonding the PDMS substrate to the lower surface of the white mica sheet by adopting a hot pressing method.
2. Performance testing
The prepared flexible piezoelectric ultrasonic transducer is tested to obtain a transmission sensitivity schematic diagram shown in fig. 5, the center frequency is 3MHz, the transmission sensitivity is 2400Pa/V, and the transmission sensitivity exceeds the reported performance (generally less than 1000 Pa/V) of the flexible transducer.
In summary, the present invention provides a high sensitivityThe flexible piezoelectric ultrasonic transducer comprises a flexible substrate, an elastic layer, a bottom electrode, a piezoelectric layer, an upper electrode and an insulating layer, wherein the piezoelectric layer is made of a piezoelectric material Ba 0.92 Ca 0.08 Ti 1-x Sn x O 3 The film has the advantages of high-voltage electrical property and no pollution, and the elastic layer is a high-temperature-resistant white mica sheet. The invention integrates ultrasonic wave transmitting and receiving functions, and the bending angle of the transducer can be smaller than 45 degrees in normal operation.
The high-sensitivity flexible piezoelectric ultrasonic transducer provided by the invention has the advantages of simple preparation method, low cost, compatibility with a microelectronic process and a piezoelectric material high-temperature annealing process, suitability for mass production, and wide application prospect in the fields of non-planar structure nondestructive inspection, biological tissue imaging, human body wearable equipment and the like.
The above-described embodiments are only preferred embodiments of the present invention and are not intended to limit the present invention. Various changes and modifications may be made by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present invention. Therefore, all the technical schemes obtained by adopting the equivalent substitution or equivalent transformation are within the protection scope of the invention.
Claims (10)
1. The utility model provides a high-sensitivity flexible piezoelectric ultrasonic transducer, includes flexible substrate, elastic layer, bottom electrode, piezoelectric layer, upper electrode and the insulating layer that have cavity structure that sets gradually, its characterized in that, the elastic layer adopts white mica sheet to prepare, and piezoelectric layer is Ba 0.92 Ca 0.08 Ti 1-x Sn x O 3 The film, x is 0.01-0.1.
2. The high-sensitivity flexible piezoelectric ultrasonic transducer according to claim 1, wherein the thickness of the elastic layer is 30 to 55 μm.
3. A highly sensitive flexible piezoelectric ultrasonic transducer according to claim 1 wherein the piezoelectric layer has a thickness of 1 to 2 μm.
4. The high-sensitivity flexible piezoelectric ultrasonic transducer according to claim 1, wherein the flexible substrate is made of a polydimethylsiloxane film, and the depth of the cavity is 200-300 μm.
5. The high-sensitivity flexible piezoelectric ultrasonic transducer according to claim 1, wherein the bottom electrode and the upper electrode are both titanium-platinum thin films, wherein the thickness of the titanium film layer in the bottom electrode is 20-30 nm, and the thickness of the platinum film layer is 200-300 nm; the thickness of the titanium film layer in the upper electrode is 10-20 nm, and the thickness of the platinum film layer is 150-180 nm.
6. The high-sensitivity flexible piezoelectric ultrasonic transducer according to claim 1, wherein the insulating layer is a silicon nitride film with a thickness of 1-2 μm.
7. A method of manufacturing a highly sensitive flexible piezoelectric ultrasound transducer according to any of claims 1 to 6, comprising the steps of:
(1) Taking a white mica sheet, and grinding and stripping the white mica sheet to obtain an elastic layer;
(2) Sequentially preparing a bottom electrode, a piezoelectric layer, an upper electrode and an insulating layer on the upper surface of the elastic layer, wherein the piezoelectric layer is composed of Ba 0.92 Ca 0.08 Ti 1-x Sn x O 3 Dripping sol on the surface of the bottom electrode, and performing spin coating, baking and annealing to form the electrode;
(3) And taking the polydimethylsiloxane film as a flexible substrate material, etching the middle area of the polydimethylsiloxane film by adopting a photolithography method to form a cavity structure, bonding the prepared flexible substrate and the lower surface of the elastic layer by adopting a hot pressing method, and covering the cavity of the flexible substrate by the elastic layer.
8. The method according to claim 7, wherein in the step (2), the baking temperature is 200 to 300 ℃ and the duration is 2 to 6 minutes; the annealing temperature is 1000-1200 ℃ and the duration time is 10-15 minutes.
9. As claimed inThe process of claim 7, wherein in step (2), the insulating layer is a silicon nitride film, silicon nitride is grown on the upper electrode by chemical vapor deposition, the gas pressure is 500-800 mTorr, the temperature is 300-450 ℃, and the reaction gas SiH 4 With NH 3 The proportion is 1:0.5 to 0.6, the reaction gas SiH 4 And N 2 The proportion is 1: 15-20.
10. The method of claim 7, wherein in step (3), the photolithography method comprises: and carrying out dry etching on the middle area of the polydimethylsiloxane film by taking photoresist as a mask, wherein the steps are carried out in a plasma etching system, and the etching parameters are as follows: 100% SF 6 The flow rate is 150-200 sccm, the power is 1200-1800W, the pressure is 0.01-0.02 mbar, the etching time is 30-40 minutes, and finally the cavity structure is formed.
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